CN109289486B - Method for separating and recovering nitrogen in high-temperature tail gas - Google Patents
Method for separating and recovering nitrogen in high-temperature tail gas Download PDFInfo
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- CN109289486B CN109289486B CN201811303374.5A CN201811303374A CN109289486B CN 109289486 B CN109289486 B CN 109289486B CN 201811303374 A CN201811303374 A CN 201811303374A CN 109289486 B CN109289486 B CN 109289486B
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- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D2256/10—Nitrogen
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Abstract
The invention discloses a method for separating and recovering nitrogen in high-temperature tail gas, which comprises the following steps: a, detecting the content of nitrogen in the high-temperature tail gas. b1 delivering the high-nitrogen tail gas with the nitrogen content of more than 90% to a first molecular sieve membrane bed, adsorbing the nitrogen in the high-nitrogen tail gas by the first molecular sieve membrane bed, and separating the gas except the nitrogen in the high-nitrogen tail gas. b2 delivering the low-nitrogen tail gas with nitrogen content less than 90% to the second molecular sieve membrane bed to adsorb the carbon dioxide in the low-nitrogen tail gas. And c, pressurizing and cooling the second gas penetrating through the second molecular sieve membrane bed, sending the second gas into a rectifying tower for rectification, and obtaining purified nitrogen according to the difference of the boiling points of the nitrogen and the oxygen. Wherein, the first molecular sieve membrane bed is selected from zeolite molecular sieves, and the second molecular sieve membrane bed is selected from 3A molecular sieves.
Description
Technical Field
The invention belongs to the field of tail gas treatment and recovery, and particularly relates to an economic and environment-friendly method for separating and recovering tail gas of a high-temperature furnace, in particular to nitrogen-containing tail gas of the high-temperature furnace.
Background
At present, purification of raw material graphite of diamond synthesis enterprises at home and abroad is dry production, most of used equipment is a high-temperature furnace, the working temperature in the furnace is generally more than 2800 ℃, and graphite has poor oxidation resistance, is particularly easy to be oxidized into carbon dioxide at high temperature to volatilize, so that the graphite purification at high temperature must be carried out in an oxygen-free environment with inert gases (such as nitrogen, argon and the like) to ensure that the graphite has higher yield and recovery rate. However, in practice, the composition of the exhaust gas discharged from the high temperature furnace is complicated due to the variation of raw materials and processes and the poor sealing effect of each valve on the furnace, and the exhaust gas from the high temperature furnace includes not only inert gas but also impurity gas containing oxygen or carbon oxide. Therefore, it is considered that the inert gas and the impurity gas are treated while the graphite product is recovered, and if the inert gas and the impurity gas are directly discharged to the air, the environment is polluted.
Therefore, it is a problem to be solved by those skilled in the art to provide a method for recycling nitrogen in the tail gas discharged from the high temperature furnace.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for separating and recovering nitrogen in high-temperature tail gas, which designs different separation and recovery modes aiming at different nitrogen contents, can obtain gases with higher purity, can recycle the gases, can reduce energy waste, is economic and environment-friendly, and has practical popularization value.
According to one aspect of the present invention, there is provided a method for separating and recovering nitrogen from high temperature tail gas, comprising: a, detecting the content of nitrogen in the high-temperature tail gas. b1 delivering the high-nitrogen tail gas with the nitrogen content of more than 90% to a first molecular sieve membrane bed, adsorbing the nitrogen in the high-nitrogen tail gas by the first molecular sieve membrane bed, and separating the gas except the nitrogen in the high-nitrogen tail gas. b2 delivering the low-nitrogen tail gas with nitrogen content less than 90% to the second molecular sieve membrane bed to adsorb the carbon dioxide in the low-nitrogen tail gas. And c, pressurizing and cooling the second gas penetrating through the second molecular sieve membrane bed, sending the second gas into a rectifying tower for rectification, and obtaining purified nitrogen according to the difference of the boiling points of the nitrogen and the oxygen. Wherein, the first molecular sieve membrane bed is selected from zeolite molecular sieves, and the second molecular sieve membrane bed is selected from 3A molecular sieves.
Optionally, step a further comprises a preparation step p: and (b) introducing the high-temperature tail gas into a solid-gas separation device, setting the temperature of the solid-gas separation device to be 800-1000 ℃, solidifying and settling part of impurity gas in the high-temperature tail gas when the impurity gas is cooled, and performing nitrogen content detection on the tail gas after impurity gas removal in the step a.
Optionally, step a further comprises a preparation step q: and d, filtering the tail gas output in the preparation step p to further remove the non-settled impurity particles doped in the tail gas, and performing nitrogen content detection on the filtered tail gas in the step a.
Optionally, in the step b1, when the nitrogen adsorption capacity of the first molecular sieve membrane bed reaches 90% -95% of the saturated nitrogen adsorption capacity, stopping introducing the high-nitrogen tail gas into the first molecular sieve membrane bed, reducing the pressure in the first molecular sieve membrane bed to 0.1-0.3 standard atmospheric pressure, desorbing the nitrogen adsorbed on the first molecular sieve membrane bed, and after the nitrogen is recovered, introducing the high-nitrogen tail gas into the first molecular sieve membrane bed again.
Optionally, in the step b2, the saturated carbon dioxide adsorption capacity of the second molecular sieve membrane bed is 10-15 mg/g, the carbon dioxide adsorption capacity of the second molecular sieve membrane bed reaches 90% -95% of the saturated carbon dioxide adsorption capacity, the low-nitrogen tail gas is stopped from being introduced into the second molecular sieve membrane bed, the pressure in the second molecular sieve membrane bed is reduced to 0.1-0.3 standard atmospheric pressure, so that the carbon dioxide adsorbed on the first molecular sieve membrane bed is desorbed, and the low-nitrogen tail gas is introduced into the second molecular sieve membrane bed again after the carbon dioxide is recovered.
Optionally, in step c, the second gas passing through the second molecular sieve membrane bed is pressurized to a pressure of 0.3-0.7MPa and the temperature is reduced to 100-.
Optionally, step c further comprises drying the pressurized and cooled second gas by concentrated sulfuric acid to remove moisture in the gas passing through the second molecular sieve membrane bed, and feeding the second gas into a rectifying tower for rectification.
Optionally, the content of nitrogen and oxygen in the second gas dried by concentrated sulfuric acid in step c is more than 99%, and the second gas is rectified in a rectifying tower to obtain purified nitrogen and purified oxygen respectively.
Optionally, further comprising step d: and c, conveying the nitrogen separated in the steps b1 and c to a nitrogen storage tank for later use.
The invention separates and recovers the tail gas of the high-temperature furnace, and prevents the tail gas from being directly discharged into the air to pollute the environment; according to the invention, two different tail gas separation and recovery methods are adopted according to the difference of the nitrogen content in the tail gas, so that the tail gas separation has pertinence, the separation effect is good, the gas with higher purity can be obtained, and the gas is recycled, thereby reducing the energy waste; in addition, the invention separates the tail gas by utilizing the different phase-change temperatures of the components of the tail gas, has good separation effect, can obtain the components of the tail gas with higher purity, is economic and environment-friendly, and has practical popularization value.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. It should be noted that, in the embodiments and examples of the present application, the feature vectors may be arbitrarily combined with each other without conflict.
A method for separating and recovering nitrogen in high-temperature tail gas comprises the following steps:
and (3) preparing step p, introducing the high-temperature tail gas into a solid-gas separation device, setting the temperature of the solid-gas separation device to be 800-1000 ℃, and allowing part of impurity gas in the high-temperature tail gas to be solidified and settled when meeting cold, enter a bottom discharger of the solid-gas separation device, and then be discharged and recovered.
And (b) preparing step q, filtering the tail gas output in the preparing step p to further remove the non-settled impurity particles doped in the tail gas, under the condition, doping part of impurity gas in the tail gas output in the preparing step p to solidify into solid fine particles when meeting cold, filtering and separating the solid fine particles from the tail gas, and feeding the filtered tail gas into the step a.
a, detecting the content of nitrogen in the tail gas.
b1 delivering the high-nitrogen tail gas with the nitrogen content of more than 90% to a first molecular sieve membrane bed, adsorbing the nitrogen in the high-nitrogen tail gas by the first molecular sieve membrane bed, and separating the gas except the nitrogen in the high-nitrogen tail gas.
b2 delivering the low-nitrogen tail gas with nitrogen content less than 90% to the second molecular sieve membrane bed to adsorb the carbon dioxide in the low-nitrogen tail gas.
c, pressurizing the second gas penetrating through the second molecular sieve membrane bed to the pressure of 0.3-0.7MPa, cooling to the temperature of 100-110K, drying the pressurized and cooled second gas by concentrated sulfuric acid to remove moisture in the second gas, and feeding the second gas into a rectifying tower for rectification.
The content of nitrogen and oxygen in the second gas dried by concentrated sulfuric acid is more than 99%, and the second gas is rectified in a rectifying tower to respectively obtain purified nitrogen and purified oxygen.
d: and c, conveying the nitrogen separated in the steps b1 and c to a nitrogen storage tank for later use.
Wherein, the first molecular sieve membrane bed is selected from zeolite molecular sieves, and the second molecular sieve membrane bed is selected from 3A molecular sieves.
And b1, wherein the saturated nitrogen adsorption capacity of the first molecular sieve membrane bed in the step b1 is 35-40% of the mass fraction of the first molecular sieve membrane bed, the nitrogen adsorption capacity of the first molecular sieve membrane bed reaches 90-95% of the saturated nitrogen adsorption capacity, the introduction of high-nitrogen tail gas into the first molecular sieve membrane bed is stopped, the pressure in the first molecular sieve membrane bed is reduced to 0.1-0.3 standard atmospheric pressure, the nitrogen adsorbed on the first molecular sieve membrane bed is desorbed, and the high-nitrogen tail gas is introduced into the first molecular sieve membrane bed again after the nitrogen is recovered.
And c, in the step b2, the saturated carbon dioxide adsorption capacity of the second molecular sieve membrane bed is 10-15 mg/g, the carbon dioxide adsorption capacity of the second molecular sieve membrane bed reaches 90% -95% of the saturated carbon dioxide adsorption capacity, the low-nitrogen tail gas is stopped being introduced into the second molecular sieve membrane bed, the pressure in the second molecular sieve membrane bed is reduced to 0.1-0.3 standard atmospheric pressure, the carbon dioxide adsorbed on the second molecular sieve membrane bed is desorbed, and the low-nitrogen tail gas is introduced into the second molecular sieve membrane bed again after the carbon dioxide is recovered.
Example 1
Introducing high-temperature furnace tail gas with the discharge capacity of 1200L/min into a solid-gas separation device with a cooling device arranged on the outer side, wherein the cooling device is internally provided with cooling circulating water, the impurity gas volatilized from graphite is solidified and settled immediately due to quenching, a discharger at the bottom of the solid-gas separation device is opened, and the solidified impurity gas is recovered at the speed of 0.056 kg/min.
And discharging the high-temperature furnace tail gas (components such as nitrogen, oxygen and the like are not solidified and still exist in a gas form) from which the impurity gas is removed through a gas outlet at the top of the solid-gas separator, introducing the high-temperature furnace tail gas into a gas analysis and measurement device for analysis and measurement, measuring the content of nitrogen in the high-temperature furnace tail gas to be 90.3%, and starting to operate the first gas recovery system (meanwhile, the second gas recovery system is in a closed state).
After entering a first filter and being filtered, the tail gas of the high-temperature furnace after analysis and measurement enters a first gas separation device comprising a first molecular sieve membrane bed, nitrogen is adsorbed in the first molecular sieve membrane bed, and other gases (such as oxygen) permeate the molecular sieve membrane bed, so that oxygen-enriched gas can be recovered.
When the nitrogen adsorbed by the first molecular sieve membrane bed reaches saturation or the separation and recovery work approaches the tail sound, the tail gas supply is stopped, the pressure in the first molecular sieve membrane bed is reduced to 0.2 standard enterprises, the nitrogen is desorbed, the purity of the recovered nitrogen is 99.5%, the recovery flow is 1029L/min, and after the nitrogen desorption is finished, the pressure in the first molecular sieve membrane bed is increased to the standard atmospheric pressure again, and the nitrogen can be continuously supplied for the separation and recovery work.
Example 2
Introducing tail gas of a high-temperature furnace with the discharge capacity of 1500L/min into a solid-gas separation device with a cooling device arranged on the outer side, wherein cooling circulating water is arranged in the cooling device, the impurity gas volatilized from graphite is solidified and settled immediately due to quenching, a discharger at the bottom of the solid-gas separation device is opened, and the solidified impurity gas is recovered at the speed of 0.07 kg/min.
And discharging the high-temperature furnace tail gas (components such as nitrogen, oxygen and the like are not solidified and still exist in a gas form) from which the impurity gas is removed through a gas outlet at the top of the solid-gas separator, introducing the high-temperature furnace tail gas into a gas analysis and measurement device for analysis and measurement, measuring the content of nitrogen in the high-temperature furnace tail gas to be 86.5%, and starting to operate a second gas recovery system (simultaneously, the first gas recovery system is in a closed state).
After entering a second filter to be filtered, the tail gas of the high-temperature furnace after analysis and measurement is sent to a gas cooling and compressing device to cool and compress the gas to ensure that the temperature is 303K and the pressure is 0.5MPa, then the tail gas after cooling and compression passes through a second molecular sieve membrane bed to adsorb carbon dioxide, finally other permeating gas permeating through the molecular sieve membrane bed is cooled to 101K through heat exchange, the permeating gas after cooling is sent to a rectifying tower to be rectified, the permeating gas is separated due to different boiling points of each component, purified nitrogen is obtained from the top of a lower tower, and purified oxygen is obtained from the bottom of an upper tower.
Wherein, the permeating gas mainly contains nitrogen and oxygen, and the nitrogen and the oxygen are in full contact with the low-temperature reflux liquid from the bottom of the lower tower from bottom to top and carry out heat transfer, so that part of the gas is condensed into liquid; because oxygen is more difficult to volatilize than nitrogen, oxygen is more condensed than nitrogen in the condensation process, so that the purity of nitrogen in the gas is improved; at the same time, the latent heat of condensation released during the condensation of the gas partially vaporizes the returning liquid, while nitrogen evaporates more than oxygen, so that the purity of oxygen in the liquid is increased.
When the gas reaches the top of the lower tower, the purity of the nitrogen in the gas phase can reach 99.999 percent (the amount is 1285 g/min); meanwhile, liquid oxygen at the bottom of the upper tower is vaporized and rises to participate in the rectification of the upper tower. Oxygen-enriched liquid (containing about 40% of oxygen) obtained from the bottom of the lower tower is fed into the upper tower, and is contacted with the ascending gas to transfer heat, wherein nitrogen is more easily vaporized, oxygen is more easily liquefied, the liquid and the ascending gas are subjected to heat and mass transfer for many times through a plurality of tower plates from top to bottom, so that the oxygen in the liquid is continuously improved, and when the liquid reaches the bottom of the upper tower, the purity of the liquid oxygen can reach 99.6%.
It is to be noted that, in this document, the terms "comprises", "comprising" or any other variation thereof are intended to cover a non-exclusive inclusion, so that an article or apparatus including a series of elements includes not only those elements but also other elements not explicitly listed or inherent to such article or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of additional like elements in the article or device comprising the element.
The above embodiments are merely to illustrate the technical solutions of the present invention and not to limit the present invention, and the present invention has been described in detail with reference to the preferred embodiments. It will be understood by those skilled in the art that various modifications and equivalent arrangements may be made without departing from the spirit and scope of the present invention and it should be understood that the present invention encompasses all modifications and equivalents within the spirit and scope of the appended claims.
Claims (3)
1. A method for separating and recovering nitrogen in high-temperature tail gas is characterized in that the method is used for treating tail gas generated in the process of producing graphite for diamond by dry purification, and the recovery method comprises the following steps:
preparation step p: introducing the high-temperature tail gas into a solid-gas separation device, setting the temperature of the solid-gas separation device to be 800-1000 ℃, and solidifying and settling part of impurity gas in the high-temperature tail gas when the impurity gas meets cold;
a preparation step q: filtering the tail gas output in the preparation step p to further remove the non-settled impurity particles doped in the tail gas;
after preparation step q, step a is performed:
step a, detecting the content of nitrogen in the high-temperature tail gas, and selecting to enter step b1 or step b2 according to the content of nitrogen in the high-temperature tail gas;
b1, conveying the high-nitrogen tail gas with the nitrogen content of more than 90% to a first molecular sieve membrane bed, adsorbing the nitrogen in the high-nitrogen tail gas by the first molecular sieve membrane bed, and separating out gases except the nitrogen in the high-nitrogen tail gas;
step b2, conveying the low-nitrogen tail gas with the nitrogen content of less than 90% to a second molecular sieve membrane bed to adsorb carbon dioxide in the low-nitrogen tail gas;
step b1 or step b2 is followed by step c: pressurizing the second gas penetrating through the second molecular sieve membrane bed to the pressure of 0.3-0.7MPa, reducing the temperature to 100-;
wherein the first molecular sieve membrane bed is selected from zeolite molecular sieves, and the second molecular sieve membrane bed is selected from 3A molecular sieves;
b1, stopping introducing high-nitrogen tail gas into the first molecular sieve membrane bed, reducing the pressure in the first molecular sieve membrane bed to 0.1-0.3 standard atmospheric pressure to desorb the nitrogen adsorbed on the first molecular sieve membrane bed, and introducing the high-nitrogen tail gas into the first molecular sieve membrane bed again after the nitrogen is recovered;
in the step b2, the saturated carbon dioxide adsorption capacity of the second molecular sieve membrane bed is 10-15 mg/g, the carbon dioxide adsorption capacity of the second molecular sieve membrane bed reaches 90% -95% of the saturated carbon dioxide adsorption capacity, the low-nitrogen tail gas is stopped being introduced into the second molecular sieve membrane bed, the pressure in the second molecular sieve membrane bed is reduced to 0.1-0.3 standard atmospheric pressure, so that the carbon dioxide adsorbed on the first molecular sieve membrane bed is desorbed, and the low-nitrogen tail gas is introduced into the second molecular sieve membrane bed again after the carbon dioxide is recovered.
2. The method for separating and recovering nitrogen from high temperature tail gas according to claim 1, wherein the content of nitrogen and oxygen in the second gas dried by concentrated sulfuric acid in step c is more than 99%, and the second gas is rectified in a rectifying tower to obtain purified nitrogen and purified oxygen respectively.
3. The method for separating and recovering nitrogen from high-temperature tail gas according to claim 1, characterized by further comprising the step d: and c, conveying the nitrogen separated in the steps b1 and c to a nitrogen storage tank for later use.
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| CN113912062A (en) * | 2021-10-09 | 2022-01-11 | 广州华糖食品有限公司 | Carbon dioxide recovery and purification process for saturated tail gas generated in sugar production by carbonic acid method |
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| US9458022B2 (en) * | 2014-03-28 | 2016-10-04 | L'Air Liquide Société Anonyme Pour L'Étude Et L'Exploitation Des Procedes Georges Claude | Process and apparatus for separating NO2 from a CO2 and NO2—containing fluid |
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| US4464188A (en) * | 1983-09-27 | 1984-08-07 | Air Products And Chemicals, Inc. | Process and apparatus for the separation of air |
| CN103787286A (en) * | 2014-03-03 | 2014-05-14 | 天津凯德实业有限公司 | Nitrogen separation and liquefaction system |
| CN108253730A (en) * | 2016-12-29 | 2018-07-06 | 天津市华赛尔气体有限公司 | A kind of air separation of nitrogen production system |
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